CN114152710A - Method for detecting total iron content in iron ore - Google Patents

Method for detecting total iron content in iron ore Download PDF

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CN114152710A
CN114152710A CN202111462633.0A CN202111462633A CN114152710A CN 114152710 A CN114152710 A CN 114152710A CN 202111462633 A CN202111462633 A CN 202111462633A CN 114152710 A CN114152710 A CN 114152710A
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周杰强
崔向鹤
赵炎
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Henan Zihuan Testing Technology Co ltd
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    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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    • G01N31/16Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • GPHYSICS
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Abstract

The invention belongs to the technical field of total iron content detection, and discloses a method for detecting total iron content in iron ore, which comprises the following steps: s1, taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and a hydrochloric acid solution, heating and stirring until the iron ore sample is completely dissolved; adding sodium bicarbonate again, stirring for dissolving, and synchronously cooling to room temperature with flowing water; sequentially adding mixed sulfuric-phosphoric acid and a manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution; s2, heating the pretreatment solution, adding a zinc chloride solution while stirring until the pretreatment solution becomes light yellow, and then continuously heating for 2 min; cooling the solution to room temperature by flowing water, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution; s3, taking a sample solution with the tungsten blue disappeared, dropwise adding an indicator diphenylamine sodium sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution becomes purple and does not fade within 30 s; and S4, calculating a result.

Description

Method for detecting total iron content in iron ore
Technical Field
The invention belongs to the technical field of total iron content detection, and particularly relates to a method for detecting total iron content in iron ore.
Background
At present, the determination of the total iron content in iron ore generally adopts a potassium dichromate titration method of mercuric chloride, the method has strong applicability and high accuracy, but mercury and chromium used in the method are toxic substances, and serious environmental pollution can be caused in the detection process, and even the body health of determination personnel is influenced.
In recent years, more and more reports on mercury-free detection methods are provided, wherein a zinc powder reduction potassium dichromate titration method is a typical mercury-free detection method, but the application and pollution of chromium are not completely eliminated by the method, so that a mercury-free and chromium-free green detection method is provided in the invention.
Disclosure of Invention
In view of this, in order to solve the problem of mercury and chromium pollution in the existing detection method, the invention aims to provide a method for detecting the content of total iron in iron ore.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for detecting the content of total iron in iron ore comprises the following steps:
s1, pretreatment
Taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and hydrochloric acid solution according to a proportion, heating and stirring until the iron ore sample is completely dissolved;
adding sodium bicarbonate again, stirring for dissolving, and synchronously cooling to room temperature with flowing water;
sequentially adding mixed sulfuric-phosphoric acid and a manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution;
s2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding a zinc chloride solution while stirring until the pretreatment solution turns light yellow, and then continuously heating for 2 min;
cooling the solution to room temperature by flowing water, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
s3. titration
Taking a sample solution with the tungsten blue disappeared, dropwise adding an indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution becomes purple and does not fade within 30 s;
s4, calculating results
Calculating the percentage content of the total iron in the iron ore,
Figure BDA0003389211390000021
in the formula:
t-total iron titration coefficient;
v, the consumption volume of the potassium permanganate standard solution in mL when the iron ore sample is titrated;
m is the mass of the iron ore sample in g.
Preferably, in the step S1, the mixing mass ratio of the iron ore sample, the sodium fluoride, the sodium bicarbonate and the hydrochloric acid solution is 2: 5: 10: 12.
preferably, in the step S1, the concentration of the hydrochloric acid solution is 1.2 g/mL.
Preferably, in the step S1, the mass ratio of the sodium bicarbonate added twice is 2: 1.
preferably, in the step S1, the addition volume ratio of the hydrochloric acid solution, the mixed phosphoric and phosphoric acid solution and the manganese sulfate solution is 2: 3: 4.
preferably, in the step S1: the sulfur-phosphorus mixed acid solution is formed by mixing a sulfuric acid solution with the concentration of 1.84g/mL and a phosphoric acid solution with the concentration of 1.7 g/mL; the concentration of the manganese sulfate solution is 150 g/L.
Preferably, in the step S2, the concentration of the zinc chloride solution is 25g/L, the concentration of the sodium tungstate solution is 250g/L, and the concentration of the titanium trichloride solution is 1.5 g/L.
Preferably, before the step S3, the potassium permanganate standard solution is added dropwise until the tungsten blue of the sample solution disappears, and the currently added potassium permanganate standard solution is not counted into the consumption volume V in the step S3.
Preferably, the sample solution is allowed to stand at room temperature until tungsten blue disappears before said step S3.
Preferably, in the step S4, the total iron titer coefficient
Figure BDA0003389211390000031
In the formula:
c (Fe) -concentration of iron standard solution in mol/L;
VT-elimination of iron standard solution upon titrationThe volume of the potassium permanganate standard solution consumed is mL.
Compared with the prior art, the invention has the following beneficial effects:
according to the detection method provided by the invention, a hydrochloric acid solution is adopted to pretreat and dissolve a sample, then zinc chloride-titanium trichloride is used for replacing mercury salt to reduce ferric iron in the pretreated solution into ferrous iron, finally sodium diphenylamine sulfonate is used as an indicator, potassium permanganate is used as a standard solution for titration detection, and a mercury-containing reagent and a chromium-containing reagent are effectively avoided in the whole detection process, so that secondary pollution of mercury and chromium to the environment is effectively eliminated.
In addition, zinc chloride and titanium trichloride are matched under an acidic medium, so that ferric iron can be completely reduced into ferrous iron, the reduction efficiency is high, the reduction effect of chloride ions on potassium permanganate is effectively inhibited, and the accuracy of a detection result is effectively improved.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Method for detecting total iron content in iron ore
S1, pretreatment
Taking 0.2g of iron ore sample, sequentially adding 0.5g of sodium fluoride, 1g of sodium bicarbonate and 10mL of hydrochloric acid solution with the concentration of 1.2g/mL, heating and stirring until the iron ore sample is completely dissolved;
adding 0.5g of sodium bicarbonate again, stirring for dissolving, and synchronously cooling to room temperature with flowing water;
mixing a sulfuric acid solution with the concentration of 1.84g/mL and a phosphoric acid solution with the concentration of 1.7g/mL to prepare a mixed sulfuric-phosphoric acid solution, sequentially adding 15mL of mixed sulfuric-phosphoric acid solution and 20mL of manganese sulfate solution with the concentration of 150g/L, and uniformly mixing to obtain a pretreatment solution.
S2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding a 25g/L zinc chloride solution while stirring until the pretreatment solution turns into light yellow, and then continuously heating for 2 min;
cooling the solution to room temperature by flowing water, dropwise adding 15 drops of sodium tungstate solution with the concentration of 250g/L, and then adding titanium trichloride solution with the concentration of 1.5g/L while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
and (3) eliminating the tungsten blue of the sample solution by dripping the potassium permanganate standard solution or standing, wherein when the potassium permanganate standard solution is dripped, the currently dripped potassium permanganate standard solution is not counted into the consumption volume V in the step S3.
S3. titration
And (3) dropwise adding 4-6 drops of indicator diphenylamine sodium sulfonate into the sample solution with the tungsten blue disappeared, then titrating the potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution becomes purple and does not fade within 30 s.
S4, calculating results
Calculating the percentage content of the total iron in the iron ore,
Figure BDA0003389211390000041
in the formula:
t-total iron titrimetric coefficient, and
Figure BDA0003389211390000042
wherein, c is the concentration of the (Fe) -iron standard solution, and the unit is mol/L; vTThe volume of potassium permanganate standard solution consumed in titrating the iron standard solution, in mL;
v, the consumption volume of the potassium permanganate standard solution in mL when the iron ore sample is titrated;
m is the mass of the iron ore sample in g.
In the above-mentioned process for obtaining the all-iron titration coefficient, an iron standard solution was prepared, and V was performed based on the same principle as the above-mentioned methodTDetection of (2):
1) preparing iron standard solution
Weighing 2.1446g of ferric oxide, placing the ferric oxide in a 200mL beaker, adding 125mL of hydrochloric acid solution with the concentration of 1.2g/mL, heating and stirring until the ferric oxide is completely dissolved; naturally cooling, adding deionized water, and adjusting the concentration of the iron standard solution to 6 mg/mL.
2) Oxidation reduction
Heating the iron standard solution to 90-100 ℃, adding a zinc chloride solution with the concentration of 25g/L while stirring until the pretreatment solution turns to light yellow, and then continuously heating for 2 min;
cooling the solution to room temperature by flowing water, dropwise adding 15 drops of sodium tungstate solution with the concentration of 250g/L, and then adding titanium trichloride solution with the concentration of 1.5g/L while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
the tungsten blue of the sample solution disappears by dripping the potassium permanganate standard solution or standing, wherein when the potassium permanganate standard solution is dripped, the currently dripped potassium permanganate standard solution is not counted into the consumption volume V in the step S3;
s3. titration
Taking a sample solution with the tungsten blue disappeared, dropwise adding 2-4 drops of indicator diphenylamine sodium sulfonate, then titrating the potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution becomes purple and does not fade within 30sT
S4, obtaining the total iron titration coefficient,
Figure BDA0003389211390000051
in the formula:
c (Fe) -concentration of iron standard solution in mol/L; vTThe volume of potassium permanganate standard solution consumed in the titration of the iron standard solution in mL.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. A method for detecting the content of total iron in iron ore is characterized by comprising the following steps:
s1, pretreatment
Taking an iron ore sample, sequentially adding sodium fluoride, sodium bicarbonate and hydrochloric acid solution according to a proportion, heating and stirring until the iron ore sample is completely dissolved;
adding sodium bicarbonate again, stirring for dissolving, and synchronously cooling to room temperature with flowing water;
sequentially adding mixed sulfuric-phosphoric acid and a manganese sulfate solution, and uniformly mixing to obtain a pretreatment solution;
s2, oxidation reduction
Heating the pretreatment solution to 90-100 ℃, adding a zinc chloride solution while stirring until the pretreatment solution turns light yellow, and then continuously heating for 2 min;
cooling the solution to room temperature by flowing water, dropwise adding a sodium tungstate solution, and then adding a titanium trichloride solution while stirring until tungsten blue appears in the pretreatment solution to obtain a sample solution;
s3. titration
Taking a sample solution with the tungsten blue disappeared, dropwise adding an indicator sodium diphenylamine sulfonate, then titrating a potassium permanganate standard solution, and recording the consumption volume V of the potassium permanganate standard solution when the sample solution becomes purple and does not fade within 30 s;
s4, calculating results
Calculating the percentage content of the total iron in the iron ore,
Figure FDA0003389211380000011
in the formula:
t-total iron titration coefficient;
v, the consumption volume of the potassium permanganate standard solution in mL when the iron ore sample is titrated;
m is the mass of the iron ore sample in g.
2. The method for detecting the content of total iron in iron ore according to claim 1, wherein the method comprises the following steps: in the step S1, the mixing mass ratio of the iron ore sample, the sodium fluoride, the sodium bicarbonate and the hydrochloric acid solution is 2: 5: 10: 12.
3. the method for detecting the content of total iron in iron ore according to claim 2, wherein the method comprises the following steps: in the step S1, the concentration of the hydrochloric acid solution is 1.2 g/mL.
4. The method for detecting the content of total iron in the iron ore according to claim 2 or 3, wherein the method comprises the following steps: in the step S1, the mass ratio of the sodium bicarbonate added twice is 2: 1.
5. the method for detecting the content of total iron in iron ore according to claim 3, wherein the method comprises the following steps: in the step S1, the addition volume ratio of the hydrochloric acid solution, the mixed sulfur and phosphoric acid solution, and the manganese sulfate solution is 2: 3: 4.
6. the method for detecting the content of total iron in iron ore according to claim 5, wherein in the step S1:
the sulfur-phosphorus mixed acid solution is formed by mixing a sulfuric acid solution with the concentration of 1.84g/mL and a phosphoric acid solution with the concentration of 1.7 g/mL;
the concentration of the manganese sulfate solution is 150 g/L.
7. The method for detecting the content of total iron in iron ore according to claim 1, wherein the method comprises the following steps: in the step S2, the concentration of the zinc chloride solution is 25g/L, the concentration of the sodium tungstate solution is 250g/L, and the concentration of the titanium trichloride solution is 1.5 g/L.
8. The method for detecting the content of total iron in iron ore according to claim 1, wherein the method comprises the following steps: before the step S3, the potassium permanganate standard solution is added dropwise until the tungsten blue of the sample solution disappears, and the currently added potassium permanganate standard solution is not counted into the consumption volume V in the step S3.
9. The method for detecting the content of total iron in iron ore according to claim 1, wherein the method comprises the following steps: before the step S3, the sample solution was allowed to stand at room temperature until tungsten blue disappeared.
10. The method for detecting the content of total iron in iron ore according to claim 1, wherein the method comprises the following steps: in the step S4, the full iron titration coefficient
Figure FDA0003389211380000021
In the formula
c (Fe) -concentration of iron standard solution in mol/L;
VTthe volume of potassium permanganate standard solution consumed in the titration of the iron standard solution in mL.
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Patent Citations (4)

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Publication number Priority date Publication date Assignee Title
CN102313771A (en) * 2010-06-29 2012-01-11 鞍钢股份有限公司 Method for determining metallic iron of iron-containing material
CN103472059A (en) * 2013-09-30 2013-12-25 武汉钢铁(集团)公司 Method for measuring total iron content in fly ash
CN104391077A (en) * 2014-12-17 2015-03-04 内蒙古包钢钢联股份有限公司 Method for determining total iron in vanadium titano-magnetite by using acid dissolution method
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